CN109289858A - Cobalt oxide and cerium dioxide composite oxide, and preparation method and application thereof - Google Patents
Cobalt oxide and cerium dioxide composite oxide, and preparation method and application thereof Download PDFInfo
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- CN109289858A CN109289858A CN201811255715.6A CN201811255715A CN109289858A CN 109289858 A CN109289858 A CN 109289858A CN 201811255715 A CN201811255715 A CN 201811255715A CN 109289858 A CN109289858 A CN 109289858A
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- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
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Abstract
The invention discloses a CoO-CeO2Composite material having a hierarchical porous structure, CoO nanoparticles and CeO2The particles have nanometer interfaces, and the specific surface area is 130m2More than g. The invention also discloses the CoO-CeO2A method for preparing a composite material and the use thereof for oxygen evolution electrodes.
Description
Technical field
The invention belongs to electrocatalysis material technical fields, and in particular to a kind of CoO-CeO2Composite oxides preparation method
And the purposes for analysing Oxygen Electrode Material.
Background technique
Analysis Oxygen Electrode Material has extensively in energy fields such as water electrolysis hydrogen production, fuel cell and metal-air batteries
Using, it has received widespread attention in recent years, however the slow dynamic process of existing analysis Oxygen Electrode Material and biggish excessively electric
Gesture limits its practical application.Currently, the analysis Oxygen Electrode Material of the prior art is mainly IrO2And RuO2Equal precious metal materials, due to
Its rare reserves, fancy price and lower stability prevent it from meet demand.Your non-gold based on transition metal
Belong to analysis Oxygen Electrode Material and carried out many researchs, especially cobalt/cobalt oxide shows analysis oxygen performance well, but it is active and steady
It is qualitative to need to be improved.
It is considered as a kind of important method for optimizing electrode material performance that surface topography, which is constructed,.Porous material has big ratio
Surface area, and it can expose its internal active component, improve atom utilization, be conducive to electrode surface and electrolyte it
Between mass transfer, be well suited for for analysing Oxygen Electrode Material.It is to set that cobalt/cobalt oxide binding function materials synthesis, which is gone out composite material,
Meter efficiently analyses the effective means of Oxygen Electrode Material, wherein CeO2In have a large amount of oxygen defects, Ce4+And Ce3+Between two states freely
Conversion has good electronic and ionic conductibility and Oxygen storage capacity, is a kind of common functional material.CeO2Work can be adjusted
Property center electronic structure, be conducive to the absorption containing oxygen intermediate generated during oxygen evolution reaction, reaction energy be effectively reduced
It builds.Therefore, by cobalt/cobalt oxide and CeO2There is the composite material of porous structure to be advantageously possible for for electrode material for design synthesis
Its performance is improved, which does not have been reported that at present.The present invention is proposed thus.
Summary of the invention
To overcome the problems, such as that existing analysis Oxygen Electrode Material is expensive, active and stability is poor, the present invention provides one kind
CoO-CeO2Compound analysis material and preparation method thereof, for analysing oxygen electrode, analysis oxygen performance has obviously to be mentioned obtained composite material
It is high.
Technical scheme is as follows:
First aspect present invention discloses a kind of CoO-CeO2Composite material, with graded porous structure, CoO nanometers
Grain and CeO2There is nano-interface between particle, specific surface area is in 130m2/ g or more.
Preferably, the classifying porous aperture is 1-50nm.
Preferably, Co/Ce atomic ratio is 0.4-2.8.
Second aspect of the present invention discloses the CoO-CeO2The preparation method of composite material, comprising the following steps:
(1) zeolite imidazole ester frame structure material is prepared, then disperses obtained zeolite imidazole ester frame structure material
Dispersion liquid is obtained in ethanol；
(2) cerium salt is dissolved in solvent, is then added in the dispersion liquid that step (1) obtains, is heated to reflux 0.5-2h, point
From being dried to obtain dried solidss after washing；
(3) dried solidss that step (2) obtains are roasted into 1-3h in reducing atmosphere to get the CoO- is arrived
CeO2Composite material.
Preferably, zeolite imidazole ester frame structure material described in step (1) is ZIF-67, preparation method are as follows: by cobalt
Salt and methylimidazole are dissolved in methanol respectively, are stood at room temperature after the two is mixed, and the solid after separating, washing is
ZIF-67；The cobalt salt is Co (NO3)3·6H2O。
Preferably, cerium salt described in step (2) is Ce (NO3)3·6H2O, the solvent are the mixture of second alcohol and water, second
The volume ratio of alcohol and water is 4:1-19:1.
Preferably, reducing atmosphere described in step (3) is hydrogen.
Preferably, maturing temperature described in step (3) is 250-500 DEG C.
Third aspect present invention discloses the CoO-CeO2Composite material is used to analyse the purposes of oxygen electrode.
Beneficial effects of the present invention:
1, CoO-CeO of the invention2Composite material has graded porous structure, and aperture is between 1-50 nanometers；Its specific surface
Product is much larger than the cobalt/cobalt oxide or CeO of one-component2, the utilization rate of the active atomic of composite material is improved, for analysing oxygen electricity
Pole can effectively facilitate the mass transfer between electrolyte and electrode surface.
2, CoO-CeO of the invention2Composite material CoO nano particle and CeO2There are a large amount of nanometers circle between nano particle
Face, for analysing oxygen electrode, by Charge transfer on interface, the electron density of active cobalt atom is greatly improved, and is more advantageous in reaction
Between product * OOH absorption, reaction energy barrier is effectively reduced.
3, CeO of the invention2In have a large amount of oxygen defects, Ce4+And Ce3+It freely converts, has good between two states
Electronic and ionic conductibility and Oxygen storage capacity, are conducive to the absorption of oxygen-containing intermediate material for analysing oxygen electrode, and electricity was reacted in reduction
Position.
4, CoO-CeO of the invention2Composite material has excellent analysis oxygen performance, is used for analysis oxygen electrode, reaches phase
It is lower than precious metal material RuO with current density overpotential needed for it2, consume less energy；The Tafel slope of curve is also below your gold
Belong to RuO2, the performance of dynamics aspect is well.In 10mA cm-250h is electrolysed under current density, overpotential rises less than 2%, stablizes
Property is excellent.
5, the present invention has the CoO- of graded porous structure and a large amount of nano-interfaces using ZIF-67 as cobalt source synthesis for the first time
CeO2Composite material, raw material sources are extensive, and synthesis path is simple, are suitble to large-scale industrial production.
Detailed description of the invention
Fig. 1 is CoO-CeO made from the embodiment of the present invention 12The scanning electron microscope sem figure of composite material.
Fig. 2 is CoO-CeO made from the embodiment of the present invention 12The high power transmission electron microscope TEM of composite material schemes.
Fig. 3 is CoO-CeO made from the embodiment of the present invention 12The graph of pore diameter distribution of composite material.
Fig. 4 is CoO-CeO made from the embodiment of the present invention 12Cobalt/cobalt oxide material obtained in composite material, comparative example 1
And commercially available CeO2The N of material2Adsorption and desorption isotherms.
Fig. 5 is CoO-CeO made from the embodiment of the present invention 12Cobalt/cobalt oxide material obtained in composite material, comparative example 1,
Commercially available CeO2Linear sweep voltammetry (LSV) figure of material and commercially available ruthinium oxide material.
Fig. 6 is CoO-CeO made from the embodiment of the present invention 12Cobalt/cobalt oxide material obtained in composite material, comparative example 1
And commercially available CeO2The Tafel curve of material and commercially available ruthinium oxide material.
Fig. 7 is CoO-CeO made from the embodiment of the present invention 12Composite material is used to analyse the stability test of Oxygen Electrode Material
Curve.
Specific embodiment
Following embodiment is intended to illustrate the content of invention, rather than further limits to the scope of the present invention.
Embodiment 1
(1) Co (NO of 0.29g is weighed3)2·6H2O and 0.65g methylimidazole is dissolved in respectively in 20mL methanol, rapidly will
The two mixes and is vigorously stirred 10min, is then stood for 24 hours at room temperature, washs two with methanol after 9000rpm centrifuge separation
It is secondary then primary with ethanol washing, ZIF-67 is obtained, then obtained ZIF-67 is dispersed in 20mL ethyl alcohol.
(2) Ce (NO of 43.4mg is weighed3)3·6H2O is dissolved in the mixed solution of 9mL ethyl alcohol and 1mL water, is vigorously stirred down
The ZIF-67 ethanol solution of 20mL is added, is heated to reflux 1h, obtains solids after being then centrifugated at 9000rpm, uses second
Alcohol washes twice solids, obtains drying solid overnight in 60 DEG C of baking ovens.
(3) solid abrasive after drying is put into tube-type atmosphere furnace at Noah's ark bottom is laid in after powder, is passed through H2/Ar
(V/V=1/9) mixed gas, first with 5 DEG C of min-1Rate be warming up to 320 DEG C then keep 2h up to CoO-CeO2Composite wood
Material.
Attached drawing 1 is CoO-CeO obtained in embodiment2The scanning electron microscope (SEM) photograph of composite material, obtains as seen from Figure 1
CoO-CeO2Composite material is accumulated by nano particle.Attached drawing 2 is CoO-CeO made from embodiment 12The high power of composite material
Transmission electron microscope picture, as seen from Figure 2 CoO nano particle and CeO2Nano-interface is formd between nano particle.Attached drawing 3 is real
Apply CoO-CeO made from example 12The graph of pore diameter distribution of composite material, there is a multiple types hole as seen from Figure 3, including micropore and
Mesoporous, aperture is between 1-50nm, based on the micropore between 1-3nm.Attached drawing 4 is CoO-CeO made from embodiment 12It is compound
The N of material2Adsorption and desorption isotherms, as seen from Figure 4 CoO-CeO made from embodiment 12The classifying porous knot of composite material
Structure makes its specific surface area reach 130m2/ g or more.
Embodiment 2
(1) preparation of ZIF-67 is the same as embodiment 1.
(2) Ce (NO of 21.7mg is weighed3)3·6H2O is dissolved in the mixed solution of 9mL ethyl alcohol and 1mL water, is vigorously stirred down
The ZIF-67 ethanol solution of 20mL is added, is heated to reflux 1h, then after 9000rpm centrifuge separation, twice with ethanol washing, 60
Drying solid is obtained overnight in DEG C baking oven.
(3) the drying solid last Noah's ark bottom that is laid in of pulverizing is put into tube-type atmosphere furnace by roasting reduction, is passed through H2/
Ar (V/V=1/9) mixed gas, first with 5 DEG C of min-1Rate be warming up to 320 DEG C then keep 2h up to CoO-CeO2Compound analysis
Material.
Embodiment 3
(1) preparation of ZIF-67 is the same as embodiment 1.
(2) Ce (NO of 86.8mg is weighed3)3·6H2O is dissolved in the mixed solution of 9mL ethyl alcohol and 1mL water, is vigorously stirred down
The ZIF-67 ethanol solution of 20mL is added, is heated to reflux 1h, then after 9000rpm centrifuge separation, twice with ethanol washing, 60
Drying solid is obtained overnight in DEG C baking oven.
(3) the drying solid last Noah's ark bottom that is laid in of pulverizing is put into tube-type atmosphere furnace by roasting reduction, is passed through H2/
Ar (V/V=1/9) mixed gas, first with 5 DEG C of min-1Rate be warming up to 320 DEG C then keep 2h up to CoO-CeO2Composite wood
Material.
Embodiment 4
(1) preparation of ZIF-67 is the same as embodiment 1.
(2) Ce (NO of 43.4mg is weighed3)3·6H2O is dissolved in the mixed solution of 9mL ethyl alcohol and 1mL water, is vigorously stirred down
The ZIF-67 ethanol solution of 20mL is added, is heated to reflux 1h, then after 9000rpm centrifuge separation, twice with ethanol washing, 60
Drying solid is obtained overnight in DEG C baking oven.
(3) the drying solid last Noah's ark bottom that is laid in of pulverizing is put into tube-type atmosphere furnace by roasting reduction, is passed through H2/
Ar (V/V=1/9) mixed gas, first with 5 DEG C of min-1Rate be warming up to 250 DEG C then keep 2h up to CoO-CeO2Composite wood
Material.
Embodiment 5
(1) preparation of ZIF-67 is the same as embodiment 1.
(2) it is heated to reflux Ce (the NO for weighing 43.4mg3)3·6H2O is dissolved in the mixed solution of 9mL ethyl alcohol and 1mL water, acute
The strong ZIF-67 ethanol solution for being added with stirring 20mL, is heated to reflux 1h, then after 9000rpm centrifuge separation, is washed with ethyl alcohol
It washs twice, obtains drying solid overnight in 60 DEG C of baking ovens.
(3) the drying solid last Noah's ark bottom that is laid in of pulverizing is put into tube-type atmosphere furnace by roasting reduction, is passed through H2/
Ar (V/V=1/9) mixed gas, first with 5 DEG C of min-1Rate be warming up to 400 DEG C then keep 2h up to CoO-CeO2Compound analysis
Oxygen elctro-catalyst.
Embodiment 6
(1) preparation of ZIF-67 is the same as embodiment 1.
(2) it is heated to reflux Ce (the NO for weighing 43.4mg3)3·6H2O is dissolved in the mixed solution of 9mL ethyl alcohol and 1mL water, acute
The strong ZIF-67 ethanol solution for being added with stirring 20mL, is heated to reflux 1h, then after 9000rpm centrifuge separation, is washed with ethyl alcohol
It washs twice, obtains drying solid overnight in 60 DEG C of baking ovens.
(3) the drying solid last Noah's ark bottom that is laid in of pulverizing is put into tube-type atmosphere furnace by roasting reduction, is passed through H2/
Ar (V/V=1/9) mixed gas, first with 5 DEG C of min-1Rate be warming up to 500 DEG C then keep 2h up to CoO-CeO2It is compound
Analyse material.
Comparative example 1
Comparative example provides one kind and CeO is not added2Cobalt/cobalt oxide one-component material, it is specific the preparation method is as follows:
(1) preparation of ZIF-67 is the same as embodiment 1.
(2) it is heated to reflux Co (the NO for weighing 29.1mg3)3·6H2O is dissolved in the mixed solution of 9mL ethyl alcohol and 1mL water, acute
The strong ZIF-67 ethanol solution for being added with stirring 20mL, is heated to reflux 1h, then after 9000rpm centrifuge separation, is washed with ethyl alcohol
It washs twice, obtains drying solid overnight in 60 DEG C of baking ovens.
(3) the drying solid last Noah's ark bottom that is laid in of pulverizing is put into tube-type atmosphere furnace by roasting reduction, is passed through H2/
Ar (V/V=1/9) mixed gas, first with 5 DEG C of min-1Rate be warming up to 500 DEG C then keep 2h up to cobalt/cobalt oxide one-component
Material.
Fig. 3 is CoO-CeO made from embodiment 12Cobalt/cobalt oxide material obtained and quotient in composite material, comparative example 1
Purchase CeO2The N of material2Adsorption and desorption isotherms comparison diagram.As seen from Figure 3, in comparative example 1 cobalt/cobalt oxide material obtained ratio
Surface area only has 65.1m2/ g, commercially available CeO2The specific surface area of material only has 9.2m2/g；And CoO-CeO made from embodiment 12It is multiple
The specific surface area of condensation material is 136.9m2/g。
Embodiment 7
The CoO-CeO that embodiment 1 is obtained2Cobalt/cobalt oxide one-component material that composite material, comparative example 1 obtain and commercially available
CeO2Material is used as analysis oxygen electrode and is tested for the property, and the substrate used is glass-carbon electrode (GCE) or nickel foam (NF), to electrode
For platinum plate electrode, reference electrode is saturated calomel electrode, and electrolyte is 1M KOH solution.As a result are as follows: the CoO- that embodiment 1 obtains
CeO2Composite material reaches 10mA cm-2Current density only need the overpotential of 319mV, Tafel slope is reduced to 63mV
dec-1, show that kinetic rate is accelerated.And the cobalt/cobalt oxide one-component material that comparative example 1 obtains is used as analysis Oxygen Electrode Material needs
The overpotential of 367mV can be only achieved 10mA cm-2Current density, Tafel slope be 67mV dec-1；Commercially available RuO2Material reaches
10mA cm-2Current density overpotential be 350mV, Tafel slope be 112mV dec-1.Therefore the CoO- that embodiment 1 obtains
CeO2Composite material analysis oxygen performance is better than cobalt/cobalt oxide and commercially available RuO that comparative example 1 obtains2Material；And commercially available CeO2Material it is anti-
Answer activity very poor, 10mA cm is still not achieved in current density when overpotential is 470mV-2, Tafel slope is 281mV dec-1,
Dynamics is very slow.As shown in attached drawing 5 and attached drawing 6.
The CoO-CeO obtained with above-mentioned condition testing example 2-62Composite material, the CoO- as a result obtained with embodiment 1
CeO2Composite material is similar.
Embodiment 8
By the condition of embodiment 7, in 10mA cm-2The result that lower continuous work 50h is obtained is as shown in Figure 7.It can be with by Fig. 7
Find out, the CoO-CeO that embodiment 1 obtains2Composite material is used as analysis oxygen electrode in 10mA cm-2It is active after lower continuous electrolysis 50h
Do not decline.And commercially available RuO2It is inactivated just very seriously after material reaction 10h, overpotential increases obvious.This illustrates that embodiment 1 obtains
CoO-CeO2Compound analysis stability of material is fine, can work long hours, and stability is better than RuO2Material has good work
Industry application prospect.
Claims (9)
1. a kind of CoO-CeO2Composite material, which is characterized in that it is with graded porous structure, CoO nano particle and CeO2Particle
Between have nano-interface, specific surface area is in 130m2/ g or more.
2. CoO-CeO according to claim 12Composite material, which is characterized in that the classifying porous aperture is 1-
50nm。
3. CoO-CeO according to claim 12Composite material, which is characterized in that Co/Ce atomic ratio is 0.4-2.8.
4. CoO-CeO according to claim 12The preparation method of composite material, which comprises the following steps:
(1) zeolite imidazole ester frame structure material is prepared, obtained zeolite imidazole ester frame structure material is then dispersed in second
Dispersion liquid is obtained in alcohol；
(2) cerium salt is dissolved in solvent, is then added in the dispersion liquid that step (1) obtains, is heated to reflux 0.5-2h, separation is washed
Dried solidss are dried to obtain after washing；
(3) dried solidss that step (2) obtains are roasted into 1-3h in reducing atmosphere to get the CoO-CeO is arrived2It is multiple
Condensation material.
5. the preparation method according to claim 4, which is characterized in that zeolite imidazole ester skeleton structure described in step (1)
Material is ZIF-67, preparation method are as follows: is dissolved in cobalt salt and methylimidazole in methanol respectively, in room temperature after the two is mixed
Lower standing, the solid after separating, washing is ZIF-67；The cobalt salt is Co (NO3)3·6H2O。
6. the preparation method according to claim 4, which is characterized in that cerium salt described in step (2) is Ce (NO3)3·
6H2O, the solvent are the mixture of second alcohol and water, and the volume ratio of second alcohol and water is 4:1-19:1.
7. the preparation method according to claim 4, which is characterized in that reducing atmosphere described in step (3) is hydrogen.
8. the preparation method according to claim 4, which is characterized in that maturing temperature described in step (3) is 250-500
℃。
9. CoO-CeO according to claim 1 to 32Composite material is used to analyse the purposes of oxygen electrode.
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Cited By (4)
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| CN110433839A (en) * | 2019-07-19 | 2019-11-12 | 华南理工大学 | A kind of preparation method for the cobalt carbon-nitrogen material loading ceria |
| CN110639530A (en) * | 2019-10-15 | 2020-01-03 | 电子科技大学 | Composite nano oxygen evolution catalyst and preparation method and application thereof |
| CN114318365A (en) * | 2022-02-11 | 2022-04-12 | 江西省科学院能源研究所 | Cobalt-vanadium-iron ternary metal water electrolysis catalyst and preparation method and application thereof |
| CN114425345A (en) * | 2020-10-15 | 2022-05-03 | 南京大学 | Co3O4/CeO2Heterojunction nanocomposite material and method of making the same |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110433839A (en) * | 2019-07-19 | 2019-11-12 | 华南理工大学 | A kind of preparation method for the cobalt carbon-nitrogen material loading ceria |
| CN110639530A (en) * | 2019-10-15 | 2020-01-03 | 电子科技大学 | Composite nano oxygen evolution catalyst and preparation method and application thereof |
| CN110639530B (en) * | 2019-10-15 | 2020-09-15 | 电子科技大学 | Composite nano oxygen evolution catalyst and preparation method and application thereof |
| CN114425345A (en) * | 2020-10-15 | 2022-05-03 | 南京大学 | Co3O4/CeO2Heterojunction nanocomposite material and method of making the same |
| CN114318365A (en) * | 2022-02-11 | 2022-04-12 | 江西省科学院能源研究所 | Cobalt-vanadium-iron ternary metal water electrolysis catalyst and preparation method and application thereof |
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| CN109289858B (en) | 2021-07-09 |
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